HRID85156

反应详情

EQUATION

反应方程式

HRID 85156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (6-(tert-butoxycarbonylamino)pyridin-3-yl)methyl methanesulfonate (102; 1.30 g, 5.4 mmol), benzyl piperazine-1-carboxylate 103; (1.42 g, 6.5 mmol), K2CO3 (2.30 g, 16.1 mmol) and NaI (0.08 g, 0.54 mmol) in DMF (20 mL) was stirred at 60° C. for 2 h. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. Water (30 mL) was added and the mixture was filtered. The collected solids were washed further with water and dried to afford benzyl 4-((6-(tert-butoxycarbonylamino)pyridin-3-yl)methyl)piperazine-1-carboxylate 104 (2.20 g, 96%).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionWater (30 mL) was added
  4. filtrationthe mixture was filtered
  5. washThe collected solids were washed further with water
  6. customdried